Advances in Sample Preparation最新文献_第8页

Curcuminoids: A multi-faceted review of green extraction methods and solubilization approaches to maximize their food and pharmaceutical applications 姜黄素：绿色提取方法和增溶途径的多方面综述，以最大限度地提高其食品和制药应用

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100159

Teshome Degfie Beshah , Mariam Araby Fekry saad , Sally el Gazar , Mohamed A. Farag

Curcuminoids, chief polyphenols in Curcuma longa L. rhizome have extensive culinary and medicinal applications. In medicine, curcuminoids exhibit potential health benefits including anticancer, antimicrobial, antitumor, antidiabetic, neuroprotective, antioxidant, and cardioprotective properties. Additionally, curcuminoids are commonly used in culinary as a spice, flavoring agent, pigment, and food additive. Considering the potential value of curcuminoids and their difficulty to be synthesized, the development of effective extraction and purification techniques for their recovery from natural sources seems warranted. To meet the demands of food and nutraceutical industries, an effective curcuminoids’ extraction process should adhere to green chemistry principles in order to ensure efficiency, safety, environmental sustainability, minimal contaminants, and cost-effectiveness. This review focuses on several curcuminoids’ separation methods including traditional techniques, such as Soxhlet, maceration, and solvent extraction, as well as green advanced technologies including ultrasound-assisted extraction, enzyme-assisted extraction, extractions via pressurized liquid, supercritical fluid, pulsed electric field, three-phase partition, and deep eutectic solvents. A comparison is presented among the different extraction methods highlighting their advantages and limitations to aid future users in deciding on the best method that suit their needs. Lastly, approaches reported on improving curcuminoids’ solubility are also presented as part of this study to enhance their bioavailability and ultimate efficacy.

姜黄素是姜黄根茎中主要的多酚类物质，具有广泛的烹饪和药用价值。在医学上，姜黄素显示出潜在的健康益处，包括抗癌、抗菌、抗肿瘤、抗糖尿病、神经保护、抗氧化和心脏保护特性。此外，姜黄素在烹饪中通常用作香料、调味剂、色素和食品添加剂。考虑到姜黄素的潜在价值及其合成的难度，开发有效的提取和纯化技术从天然来源中回收姜黄素似乎是必要的。为了满足食品和营养保健行业的需求，有效的姜黄素提取工艺应遵循绿色化学原则，以确保效率、安全性、环境可持续性、最小污染物和成本效益。综述了姜黄素的几种分离方法，包括索氏法、浸渍法、溶剂萃取法等传统方法，以及超声辅助萃取法、酶辅助萃取法、加压液萃取法、超临界流体萃取法、脉冲电场萃取法、三相萃取法、深共晶溶剂萃取法等绿色先进技术。对不同的提取方法进行了比较，突出了它们的优点和局限性，以帮助未来的用户决定适合他们需要的最佳方法。最后，本研究还介绍了改善姜黄素溶解度的方法，以提高其生物利用度和最终疗效。

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引用次数: 0

Sustainable Supramolecular Deep Eutectic Solvents based extraction for bioactive phenolic compounds recovery from olive pomace 基于可持续超分子深共晶溶剂的萃取技术，用于从橄榄渣中回收生物活性酚类化合物

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100166

G. Pietrangeli , S. Della Posta , E. D'Alessandro , S.M. Giannitelli , M. Trombetta , C. Maggi , L. De Gara , C. Fanali

Olive oil industries produce a large quantity of by-product, such as wastewater and olive pomace, which are characterized by a high concentration of phenolic compounds, which can be recovered and eventually reused in cosmeceutical and nutraceutical fields. The recovery of bioactive molecules from waste is usually carried out by common of organic solvents. To respect the principles of green chemistry, other solvents such as Deep Eutectic Solvents (DESs) have been evaluated. DESs are sustainable solvents involved in sample preparation. Recently, DESs have also been evaluated as extraction solvent with the addition of β-cyclodextrins (β-CDs) which are cyclic oligosaccharide molecules obtained from the enzymatic degradation of starch, and their characteristics allow them to be selective toward certain analytes. These innovative solvents, called Supramolecular Deep Eutectic Solvents (SupraDESs), seem to be excellent green solvents for the extraction of phenolic compounds and are a sustainable alternative to conventional solvents. The aim of this work was to develop and optimize an analytical procedure for the extraction of phenolic compounds from olive pomace, using a SupraDES composed by ammonium acetate - lactic acid (in a molar ratio of 1:7) with the addition of a certain amount of β-cyclodextrins as extraction solvent. The optimized extraction procedure, defined through Box-Behnken Design, is based on the best extraction time of 22 min, temperature of 43°C, solid-to-liquid ratio of 1:48 (g:mL) and β-CDs concentration of 1.8 % (w/w). The qualitative profile of the extracted phenolic compounds was determined through high performance liquid chromatography coupled with mass spectrometry.

橄榄油工业产生大量的副产品，如废水和橄榄渣，其特点是高浓度的酚类化合物，这些副产品可以回收并最终用于药妆和营养保健领域。从废物中回收生物活性分子通常是用普通的有机溶剂进行的。为了尊重绿色化学的原则，其他溶剂，如深共晶溶剂（DESs）已被评估。DESs是用于样品制备的可持续溶剂。最近，DESs也被评价为添加β-环糊精（β-CDs）的萃取溶剂，β-环糊精是一种从淀粉酶降解中获得的环状低聚糖分子，它们的特性使它们对某些分析物具有选择性。这些创新的溶剂，被称为超分子深共晶溶剂（SupraDESs），似乎是萃取酚类化合物的优秀绿色溶剂，是传统溶剂的可持续替代品。本研究的目的是建立并优化一种从橄榄渣中提取酚类化合物的分析方法，采用醋酸铵-乳酸（摩尔比为1:7）组成的SupraDES，加入一定量的β-环糊精作为提取溶剂。通过Box-Behnken设计确定最佳提取工艺，最佳提取时间为22 min，温度为43℃，料液比为1:48 (g:mL)， β-CDs浓度为1.8% （w/w）。采用高效液相色谱-质谱联用技术对提取的酚类化合物进行定性分析。

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引用次数: 0

Greener solvents for microelution solid phase extraction of proteins from biological fluids followed by their top-down CE-MS analysis 更环保的微洗脱溶剂，固相萃取生物液中的蛋白质，然后进行自上而下的CE-MS分析

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100160

Martina Opetová , Radovan Tomašovský , Katarína Maráková

In recent years, there has been a growing demand for making the analytical processes sustainable and environmentally friendly. In proteomic analysis, sample preparation plays an important role, employing different extraction techniques to isolate proteins of interest from biological fluids to be able to analyze them. These techniques usually use large volumes of organic solvents, such as acetonitrile, which has been recognized as hazardous and difficult to dispense. According to green analytical chemistry principles, the environmental impact of the methods can be reduced either by miniaturizing the processes or by replacing organic solvents with less toxic alternatives. This work compares the effect of different greener solvents on the solid-phase extraction process of low molecular weight proteins spiked in biological fluids (pooled human serum, plasma, urine, and saliva) and suggests that ethanol (60 %, v/v) offers, when used as an elution solvent, comparable results to acetonitrile (75 % v/v) in terms of extraction recovery. The addition of acidic modifiers to the elution solvent did not improve the extraction recovery, and the nitrogen evaporation of the eluate resulted in a 17–53 % loss of the proteins compared to the simple dilution of the eluate.

近年来，越来越多的人要求使分析过程具有可持续性和环境友好性。在蛋白质组学分析中，样品制备起着重要的作用，采用不同的提取技术从生物流体中分离出感兴趣的蛋白质，以便能够分析它们。这些技术通常使用大量的有机溶剂，如乙腈，这是公认的危险和难以分配。根据绿色分析化学原理，这些方法对环境的影响可以通过将过程小型化或用毒性较小的替代品取代有机溶剂来减少。本研究比较了不同绿色溶剂对生物液体（混合的人血清、血浆、尿液和唾液）中低分子量蛋白质固相萃取过程的影响，并表明乙醇（60%,v/v）作为洗脱溶剂时，提取回收率与乙腈（75% v/v）相当。在洗脱溶剂中加入酸性改性剂并没有提高萃取回收率，与简单稀释洗脱液相比，洗脱液的氮蒸发导致蛋白质损失17 - 53%。

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引用次数: 0

Automated capillary electrophoresis analyses of dried blood samples after patient-centric volumetric absorptive microsampling 以病人为中心的体积吸收显微取样后干血样的自动毛细管电泳分析

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2024.100142

Richard Maršala , Miloš Dvořák , Pavel Kubáň

An automated method for the analysis of dried blood samples collected by volumetric absorptive microsampling (VAMS) is presented for the first time. A single commercial capillary electrophoresis (CE) instrument (with no need for hardware or software modifications) was employed for the expeditious analyses of the dried material using several integral and novel features. These included the use of external pressure for sub-minute sample preparation from Mitra® VAMS polymeric tips, the use of the sampling tips as inherent micro-agitators for instant eluate homogenization, preparation/sampling at the CE outlet for more convenient capillary length adjustment, and short-end injection for sub-minute CE separation and quantification of lactate as a model analyte.

The operational parameters for the sample preparation and analysis were comprehensively evaluated resulting in a baseline separation of lactate from all endogenous matrix compounds. The optimized method demonstrated excellent intra- and inter-day repeatability of peak areas (RSD values ≤ 7.2 %), linearity (R² = 0.9990) over the clinically relevant concentration range (0.15 – 20 mM), the limits of detection and quantification at 0.03 and 0.1 mM, respectively, and a sample throughput ≥ 16 samples/hour. No ageing was observed for VAMS devices stored at ambient conditions for up to 14 days. Comparative analysis with a portable lactate analyser revealed slightly elevated concentrations in dried vs. liquid capillary blood due to the glycolysis of glucose during drying, nevertheless, lactate concentrations in Mitra® devices correlated well with those in blood plasma, which is typically used in clinical practice.

The present study offers a robust, accurate, and environmentally benign concept for the automated analyses of VAMS-collected blood samples with its potential application in patient-centric sampling, clinical diagnostics and research, and personalized healthcare.

首次提出了一种自动分析容量吸收微采样（VAMS）采集的干血样本的方法。一个单一的商用毛细管电泳（CE）仪器（不需要硬件或软件修改）被用于快速分析干燥的材料使用几个完整的和新颖的特征。这些包括使用外部压力从Mitra®VAMS聚合物尖端制备亚分钟样品，使用取样尖端作为固有的微搅拌器进行即时洗脱均质，在CE出口制备/取样以更方便地调整毛细管长度，以及短端注射用于亚分钟CE分离和乳酸作为模型分析物的定量。对样品制备和分析的操作参数进行了全面评估，从而从所有内源性基质化合物中分离出乳酸盐。优化后的方法具有良好的峰面积内和日间重复性（RSD值≤7.2%），在临床相关浓度范围（0.15 ~ 20 mM）内线性（R²= 0.9990），检出限和定量限分别为0.03和0.1 mM，样品通量≥16个样品/小时。VAMS设备在环境条件下储存长达14天，未观察到老化。与便携式乳酸分析仪的比较分析显示，由于干燥过程中葡萄糖的糖酵解，干燥毛细血管血液中的乳酸浓度与液体毛细血管血液中的乳酸浓度略有升高，然而，Mitra®设备中的乳酸浓度与血浆中的乳酸浓度具有良好的相关性，这通常用于临床实践。本研究为vams采集的血液样本的自动分析提供了一个可靠、准确和环保的概念，并具有在以患者为中心的采样、临床诊断和研究以及个性化医疗保健方面的潜在应用。

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引用次数: 0

DES modified silica gel as dispersing material for miniaturized matrix solid phase dispersion applied to triazoles determination DES改性硅胶作为分散材料，用于三唑类化合物的微型基质固相分散测定

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100153

Susanna Della Posta , Valeria Gallo , Emanuele Limiti , Marcella Trombetta , Monica Gherardi , Alessandra Gentili , Laura De Gara , Chiara Fanali

Matrix solid phase dispersion (MSPD) represents one of the most useful methods for pesticides determination in vegetables. This extraction method involves the use of a solid, dispersing material, which is homogenized together with the sample in a mortar and loaded into a cartridge for the analyte's elution with a suitable solvent. Innovative MSPDs involve the use, as dispersing material, of silica gel (SCG) impregnated with deep eutectic solvents (DESs). SCG high porosity can facilitate DES impregnation process due to hydrogen bonds or electrostatic interactions among them.

A miniaturized MSPD extraction for triazoles from tomato using as dispersant DES modified SCG, followed by HPLC-MS extracts analysis, was developed. Four DES modified SCGs were tested in the MSPD procedure and the best result in terms of extracted triazoles was obtained using a choline chloride – Propylene Glycol DES modified SCG. Ethyl Acetate was selected as MSPD procedure extractive solvent resulting more efficient than methanol, acetonitrile and chloroform. The optimization of the extraction procedure involved the study of SCG to DES ratio (w/v), sample to dispersing material ratio (w/w) and extractive solvent volume able to obtain the greatest recovery of triazoles from tomato. The optimized method was validated and maximum values of 3.6 % and 8.3 % were obtained for intra-day and inter-day precision respectively. For each analyte the calculated limit of quantification was similar or lower than their Maximum Residue Limit. Triazoles mean recovery ranged from 70 to 102 %.

The new ChCl-propylene glycol DES modified SCG represents a valid alternative to conventional dispersing material in MSPD procedure apply to pesticides determination.

基质固相分散法（MSPD）是蔬菜中农药含量测定中最有用的方法之一。这种提取方法包括使用固体分散材料，该材料与样品一起在砂浆中均质，并装入一个用合适溶剂洗脱分析物的药筒中。创新的mspd包括使用浸渍有深共晶溶剂（DESs）的硅胶（SCG）作为分散材料。SCG的高孔隙率可以通过氢键或静电相互作用促进DES浸渍过程。研究了以DES改性SCG为分散剂的微型MSPD提取番茄中三唑的方法，并对提取物进行了HPLC-MS分析。用MSPD法对四种DES修饰的SCG进行了测试，氯胆碱-丙二醇DES修饰的SCG提取三唑的效果最好。选择乙酸乙酯作为MSPD萃取溶剂，萃取效率高于甲醇、乙腈和氯仿。优化提取工艺，考察SCG / DES比（w/v）、样品与分散物比（w/w）和萃取溶剂体积对番茄中三唑提取率的影响。对优化后的方法进行了验证，得到的日内精密度最大值为3.6%，日内精密度最大值为8.3%。每种分析物的定量计算限与最大残留限相近或低于其最大残留限。三唑类药物的平均回收率为70% ~ 102%。新型氯丙二醇DES改性SCG代表了一种有效的替代传统分散材料的MSPD方法在农药测定中的应用。

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引用次数: 0

The solvent-assisted dispersive solid-phase extraction method revisited. Application for the determination of anionic surfactants 对溶剂辅助分散固相萃取法进行了研究。阴离子表面活性剂的测定方法

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100162

Serhii Zaruba , Patrycja Makoś-Chełstowska , Vasil Andruch

A new approach in solvent-assisted dispersive solid-phase extraction (SA-DSPE) procedure using a supercooled liquid was developed. It demonstrates the first use of a supercooled liquid in this technique, in particular, and in chemical analysis in general. Moreover, to the best of our knowledge, this is the first work devoted to the determination of the total concentration of anionic surfactants (as LAS, Linear alkylbenzene sulfonate) using a micro-SPE technique. The method is based on the formation of an ion pair between astraphloxine (cationic dye) and an anionic surfactants, with subsequent extraction of the ion pair formed onto a benzophenone sorbent generated in situ after injection of its 5 % solution in an acetone:water 80:20 v/v mixture into an aqueous sample. The resulting turbidness was sedimented by centrifugation. The addition of a few crystals of benzophenone then leads to the solidification of a supercooled solution of the sorbent, which facilitates the separation. Afterwards, the bulk of the aqueous phase was easily decanted, and the resulting sediment was dissolved with 500 μL of acetone; absorbance measurements were carried out in a semi-microcuvette. The calibration plot was linear up to 0.5 µmol L⁻¹ of sodium dodecylbenzene sulfonate (SDBS). The LOD and LOQ, were 9.0 and 30 nmol L^-1 of SDBS, respectively. The developed procedure was applied for the determination of anionic surfactants in various real water samples.

提出了一种利用过冷液体进行溶剂辅助分散固相萃取（SA-DSPE）的方法。它展示了在这种技术中，特别是在化学分析中首次使用过冷液体。此外，据我们所知，这是第一个致力于用微spe技术测定阴离子表面活性剂（如LAS，线性烷基苯磺酸盐）总浓度的工作。该方法是基于在黄芪（阳离子染料）和阴离子表面活性剂之间形成离子对，随后将其在丙酮：水80:20 v/v混合物中注射5%溶液后原位生成的二苯甲酮吸附剂上形成的离子对萃取到含水样品中。所得浊度通过离心沉淀。加入一些二苯甲酮晶体会导致吸附剂的过冷溶液凝固，从而促进分离。之后，将大部分水相轻松滗出，用500 μL丙酮溶解所得沉积物；在半微比色皿中进行吸光度测量。校正图在十二烷基苯磺酸钠（SDBS）浓度为0.5µmol L−1时呈线性关系。sds的LOD和LOQ分别为9.0和30 nmol L-1。该方法可用于各种实际水样中阴离子表面活性剂的测定。

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引用次数: 0

Application of deep eutectic solvents for the determination of inorganic analytes 深共晶溶剂测定无机分析物的应用

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100158

Vasil Andruch , Viera Vojteková , Alina Kalyniukova , Gokhan Zengin , Ingrid Hagarová , Tanya Yordanova

Deep eutectic solvents (DESs), due to their unique physicochemical properties, such as low volatility, tunable viscosity, and excellent solvation capabilities, have emerged as promising alternatives to conventional solvents in the determination of inorganic analytes. This work comprises various DES compositions that effectively improve the sensitivity, selectivity, and environmental sustainability of analytical procedures for the determination of inorganic analytes. DESs crucially take part in extraction, preconcentration, and digestion processes, followed by measurements with atomic absorption spectrometry, plasma-based techniques, UV–Vis spectrophotometry, etc. This work aims to reveal their great potential in the field of elemental analysis for the determination of inorganic analytes in various types of samples. Furthermore, the challenges and limitations associated with the use of DESs, including matrix effects, viscosity issues and compatibility with analytical instrumentation, are critically evaluated.

深共晶溶剂（DESs）由于其独特的物理化学性质，如低挥发性、可调粘度和优异的溶剂化能力，已成为测定无机分析物的传统溶剂的有希望的替代品。这项工作包括各种DES组成，有效地提高了测定无机分析物的分析方法的灵敏度、选择性和环境可持续性。DESs在萃取、预浓缩和消化过程中起着至关重要的作用，随后使用原子吸收光谱法、等离子体技术、紫外可见分光光度法等进行测量。这项工作旨在揭示它们在元素分析领域的巨大潜力，用于测定各种类型样品中的无机分析物。此外，与DESs使用相关的挑战和限制，包括基质效应，粘度问题和与分析仪器的兼容性，进行了批判性评估。

引用次数: 0

Advances in applications of metal-organic frameworks for selective solid-phase extraction and chromatographic separation of active pharmaceutical ingredients 金属-有机骨架在药物活性成分选择性固相萃取和色谱分离中的应用进展

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100151

Zhenyu Song , Bodong Liu , Zezhou Zang , Zeyi Li , Ying Jiang , Tiantian Si , Min Sun

Active pharmaceutical ingredients (APIs) constitute a fundamental component in the development and clinical application of pharmaceuticals, thereby playing an indispensable and pivotal role within the realm of biomedicine. In current research, metal-organic frameworks (MOFs) have garnered considerable attention for studying APIs, serving as effective adsorbents for the extraction of APIs or as stationary phases for their separation. Notably, MOFs composites have significantly enhanced the enrichment and selectivity for APIs by modifying their size, micropore structure, surface characteristics, and charge. The mechanisms underlying these improvements include hydrogen bonding, π-stacking interactions, electrostatic interactions, hydrophobic interactions, and hydrophilic interactions. This comprehensive review focuses on the latest advancements and breakthroughs in the application of MOFs for selective extraction, enrichment, and chromatographic separation of APIs within solid-phase extraction, solid-phase microextraction, and chromatographic stationary phases spanning the period from 2020 to 2024. Additionally, the review highlights the potential development of MOFs in sample preparation chromatographic separation for application, particularly for APIs derived from traditional Chinese medicine (TCM), providing valuable insights into the research and development of nanomaterials such as MOFs in using APIs.

活性药物成分是药物开发和临床应用的基础成分，在生物医学领域中起着不可或缺的关键作用。在目前的研究中，金属有机骨架（MOFs）作为有效的吸附剂用于原料药的提取或作为固定相用于原料药的分离，在原料药的研究中受到了广泛的关注。值得注意的是，mof复合材料通过改变其尺寸、微孔结构、表面特征和电荷，显著提高了原料药的富集和选择性。这些改进的机制包括氢键、π堆积相互作用、静电相互作用、疏水相互作用和亲水相互作用。本文综述了2020年至2024年mof在固相萃取、固相微萃取和色谱固定相中选择性提取、富集和色谱分离原料药的最新进展和突破。此外，本文还强调了mof在样品制备色谱分离中的应用潜力，特别是在中药原料药的应用方面，为mof等纳米材料在原料药应用方面的研究和开发提供了有价值的见解。

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引用次数: 0

Greener and rapid magnetic solid phase microextraction method using Fe3O4@Al2O3/AC for chromatographic determination of neonicotinoid pesticides in vegetable oils 绿色快速的Fe3O4@Al2O3/AC磁固相微萃取法测定植物油中新烟碱类农药

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100152

Musiiwa V. Sengane , Masixole Sihlahla , Philiswa N. Nomngongo , Nomvano Mketo

A greener sample preparation method based on magnetic solid phase microextraction (MSPμE) was developed for the preconcentration of neonicotinoid pesticides (acetamiprid, imidacloprid, thiacloprid and thiamethoxam) in vegetable oil samples followed by separation and quantification using high performance liquid chromatography with diode array detector (HPLC-DAD). Different characterisation techniques such as Fourier Transform Infrared Spectroscopy (FTIR), Powder X-ray diffraction analysis (PXRD), Thermogravimetric Analysis (TGA), Transmission electron microscopy (TEM), and scanning electron microscope and energy-dispersive X-ray spectroscopy (SEM-EDS) confirmed the synthesised magnetic nano adsorbents (Fe₃O₄, Fe₃O₄@Al₂O₃ and Fe₃O₄@Al₂O₃/AC). The most influential parameters affecting MSPμE of NEOs by Fe₃O₄@Al₂O₃/AC were examined using a multivariate optimisation approach and 8 min extraction time, 13 pH, 9 mg adsorbent mass, and 0.5 mL eluent volume were optimal parameters. The proposed Fe3O4@Al2O3/AC method showed high accuracy (80–119.21%) and precision (≤10 %) for all the investigated NEOs. Additionally, the obtained limit of detection (LOD) ranged from 0.5–1.76 ng µL^-1, the limit of quantification (LOQ) ranged from 1.87–6.62 ng µL^-1 and satisfactory high preconcentration factors (73.02- 407.0) were comparable with literature reported studies. The Analytical GREEness calculator AGREE, BAGI and NEMI analysis confirmed greenness of MSPμE. After that, the validated MSPμE method was applied to real vegetable oil samples (avocado, canola, olive and sunflower), and fortunately, all the investigated NEOs were below LODs of the proposed MSPμE /HPLC-DAD methods.

建立了一种基于磁固相微萃取（MSPμE）的绿色样品制备方法，用于植物油样品中新烟碱类农药（啶虫脒、吡虫啉、噻虫啉和噻虫嗪）的预富集，并采用高效液相色谱二极管阵列检测器（HPLC-DAD）进行分离和定量。不同的表征技术，如傅里叶变换红外光谱（FTIR），粉末x射线衍射分析（PXRD），热重分析（TGA），透射电子显微镜（TEM），扫描电子显微镜和能量色散x射线能谱（SEM-EDS）证实了合成的磁性纳米吸附剂（Fe3O4， Fe3O4@Al2O3和Fe3O4@Al2O3/AC）。采用多元优化方法考察了Fe3O4@Al2O3/AC法提取neo的MSPμE的影响因素，确定提取时间为8 min， pH为13，吸附剂质量为9 mg，洗脱液体积为0.5 mL。所提出的Fe3O4@Al2O3/AC方法对所研究的近地天体具有较高的准确度（80-119.21%）和精密度（≤10%）。检出限（LOD）为0.5 ~ 1.76 ngµL-1，定量限（LOQ）为1.87 ~ 6.62 ngµL-1，高富集系数（73.02 ~ 407.0）与文献报道的研究相当。分析绿色计算器AGREE、BAGI和NEMI分析证实了MSPμE的绿色度。然后，将验证的MSPμE方法应用于实际植物油样品（牛油果、菜籽油、橄榄和向日葵），幸运的是，所有检测的neo都低于所建立的MSPμE /HPLC-DAD方法的lod。

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引用次数: 0

New trends in bioanalysis sampling and pretreatment: How modern microsampling is revolutionising the field 生物分析采样和预处理的新趋势：现代微采样如何彻底改变该领域

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100161

Michele Protti , Elisa Milandri , Roberta Di Lecce , Laura Mercolini , Roberto Mandrioli

Microsampling technologies are revolutionising bioanalysis by enabling minimally invasive, decentralized sample collection, offering significant advantages over traditional methods in terms of patient compliance, cost-effectiveness, and analytical efficiency. This review explores the latest advancements in microsampling devices, including microfluidic and quantitative dried blood spot systems (mfDBS and qDBS, respectively), calibrated capillary-based devices, volumetric absorptive microsampling (VAMS) technologies, microneedle-based microsampling, radial-based DBS devices, membrane-based plasma separation technologies and vacuum-assisted blood collection systems. By addressing pre-analytical variability, enhancing analyte stability, and supporting decentralized workflows, these technologies align with modern and green analytical chemistry principles. The unique capabilities of these emerging microsampling technologies and devices further demonstrate their transformative potential. However, challenges remain, including haematocrit dependency for some parameters, user variability, and standardisation across devices. This review highlights ongoing innovations and their implications for expanding to high-quality bioanalytical testing.

微采样技术通过实现微创、分散的样本采集，正在彻底改变生物分析，在患者依从性、成本效益和分析效率方面比传统方法具有显着优势。本文综述了微采样设备的最新进展，包括微流控和定量干血点系统（分别为mfDBS和qDBS），校准毛细管设备，体积吸收微采样（VAMS）技术，微针微采样，径向DBS设备，膜等离子体分离技术和真空辅助采血系统。通过解决分析前的可变性，增强分析物的稳定性，并支持分散的工作流程，这些技术符合现代和绿色分析化学原则。这些新兴的微采样技术和设备的独特功能进一步展示了它们的变革潜力。然而，挑战仍然存在，包括对某些参数的红细胞压积依赖，用户可变性和跨设备的标准化。这篇综述强调了正在进行的创新及其扩展到高质量生物分析测试的意义。

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